反应详情

A mixed solution of colchicine (5.00 g, 12.5 mmoles), an aqueous 40% methylamine solution (10 ml, 130 mmol) and ethyl alcohol (10 ml) was subjected to reaction at 120° C. for 20 hours under stirring in a sealed tube. The solvent was distilled off, water (10 ml) was added to the residue, and the mixture was extracted with chloroform. The chloroform layer was separated, washed with water and dried. The solvent was evaporated, and the residue was separated and purified by silica gel column chromatography [chloroform:methanol (20:1)]. Thereby, 4.18 g of N-methylcolchiceinamide was obtained as yellow crystals (yield 84%) . ##STR17##

1. distillationThe solvent was distilled off
2. additionwater (10 ml) was added to the residue
3. extractionthe mixture was extracted with chloroform
4. customThe chloroform layer was separated
5. washwashed with water
6. customdried
7. customThe solvent was evaporated
8. customthe residue was separated
9. custompurified by silica gel column chromatography [chloroform:methanol (20:1)]